反应详情

温度

120 °C

A mixture of 4-chlorobenzylamine (1 mL) and methyl 4-hydroxy-1-benzothiophene-5-carboxylate (Preparation 13, 0.50 g) is heated to 120° C. under an atmosphere of nitrogen for 4 hours. After cooling, the residue is diluted with ethyl acetate and methanol (1:1) and absorbed onto silica gel. Chromatography on a Biotage column eluting with 500 mL of toluene gave 520 mg (68%) of the title compound as a white solid. Physical characteristics: Mp 168-169° C.; MS (ESI−) m/z 316.1 (M−H)−. Anal. Found: C, 60.82; H, 3.87; N, 4.33.

1. temperatureAfter cooling
2. customabsorbed onto silica gel
3. washChromatography on a Biotage column eluting with 500 mL of toluene